CN102775192A - Seed crystal introduced agate red ceramic pigment and preparation method thereof - Google Patents
Seed crystal introduced agate red ceramic pigment and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a seed crystal introduced agate red ceramic pigment and a preparation method of the seed crystal introduced agate red ceramic pigment. The preparation method comprises the following steps of: (1) preparing seed crystals: evenly mixing calcium carbonate, stannic oxide, quartz and chrome green according to a molar ratio of (0.9-1.1):(0.9-1.1):(0.9-1.1):(0.115-0.135), mixing and grinding the obtained mixture, agate ball stone and water according to proportion by weight of 100:(450-550):(54-66) until the grain size achieves D90<=5mu m, drying and sieving the ground mixture, then adding boron-contained compounds which are 3%-5% of total weight, evenly mixing, burning, grinding and drying to obtain the seed crystals; and (2) preparing the pigment: evenly mixing calcium carbonate, stannic oxide, quartz and chrome green according to a molar ratio of (0.9-1.1):(0.9-1.1):(0.9-1.1):(0.115-0.135), adding the seed crystals which are 1%-3% of the total weight and the boron-contained compounds which are 3%-5% of the total weight, evenly mixing, burning, grinding and drying to obtain end products. The seed crystal introduced agate red ceramic pigment and the preparation method can reduce synthetic difficulties of the pigment and are strong in color development, bright in color and luster and good in thermostability.
Description
Technical field
The present invention relates to the production technical field of ceramic pigment, relate in particular to a kind of agate red ceramic pigment of introducing crystal seed and preparation method thereof.
Background technology
Chrome tin pink is claimed agate red again, is a kind of pyroceramic colorant, because this colorant has stable crystalline structure, thereby in the parent glaze that adapts to, can demonstrate beautiful agate red.Chrome tin pink is used for wall brick, floor tile, sanitary china can be obtained good decoration effect, thereby be one of widely used colorant in present top-grade building, the sanitary china goods.
But for a long time, people seem quite weak to the research of the synthesis mechanism of agate red ceramic pigment, and to influence its synthetic factor very complicated again in addition, as long as certain link of intermediary has mistake slightly, all will influence the quality of final colorant.Therefore, the synthesis mechanism of research agate red ceramic pigment and the factor of the main colour generation of influence are confirmed best production process system, have crucial meaning.
In the production process of agate red ceramic pigment; The synthetic difficulty of agate red ceramic pigment is mainly reflected in complexity and the inlet that chromium gets into its aspidelite type lattice, and the quantity that chromium gets into tin tip stone is many more, and colour generation better; It is easy more that chromium gets into tin tip stone lattice, and synthesis technique is just got over easy handling.
Summary of the invention
In view of this, the objective of the invention is to, a kind of preparation method who introduces the agate red ceramic pigment of crystal seed is provided, increase the resultant velocity of colorant, promote tin tip stone to generate, promote chromium to get into tin tip stone lattice through introducing crystal seed.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of preparation method who introduces the agate red ceramic pigment of crystal seed comprises the steps:
1) crystal seed preparation:
With lime carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes, mixture; With mixture and agate ballstone, water by 100: (450～550): the weight ratio of (54～66) is mixed, is ground, and reaches D until particle diameter
90≤5um, the mixture after will grinding again carries out drying, sieves, and then adds the boron-containing compound mixing account for gross weight 3%～5%, then calcines, grinds, drying, obtains crystal seed;
2) colorant preparation:
With lime carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes; Add the boron-containing compound that accounts for crystal seed gross weight 1%-3%, that step 1) makes and account for gross weight 3%～5% again; Calcining behind the mixing, grinding, drying get product.
Preferably, step 1) and step 2) in, the mol ratio of lime carbonate, tindioxide, quartz, chrome green is 1: 1: 1: 0.125.
Preferably, step 1) and step 2) in the ball milling of grinding for adopting ball mill to carry out.
Preferably, the incinerating processing condition are in the step 1): 30 ℃～500 ℃, and intensification 4H; 500 ℃～1000 ℃, intensification 4H; 1000 ℃～(1200-1300 ℃), intensification 5H; At 1200 ℃～1300 ℃ following constant temperature 5H, cooling naturally then.
Preferably, step 2) the incinerating processing condition are in: 30 ℃～500 ℃, and intensification 4H; 500 ℃～1000 ℃, intensification 4H; 1000 ℃～1200 ℃, intensification 3H; 1200 ℃ of following constant temperature 4H then are cooled to below 200 ℃ naturally.
Preferably, step 1), step 2) in drying all carrying out below 150 ℃.
Preferably, step 1) and step 2) in, the water ratio of dry back mixture is less than 0.5%.
Preferably, in the step 1), calcine is ground to particle diameter D in the calcining back
90Reach 3～5mm.
Preferably, step 2) in, calcine is ground to particle diameter D in the calcining back
90Be 16mm～20mm.
Agate red ceramic pigment of the present invention is made by aforementioned preparation method.
Compared with prior art, the present invention is owing to introduce crystal seed in the preparation process of agate red ceramic pigment, and changes the fineness activity and the mixture homogeneity of raw material during the preparation crystal seed through the mode of ball milling refinement; Because when pressed powder mixes; Less than the material that accounts for total amount 1% is to be difficult to go in the system of evenly spreading to, and the mode through the ball milling refinement makes material uniform distribution such as chromic oxide and fineness reach refinement, through calcining high temperature solid state reaction takes place more easily according to the uniform material of solid state reaction mechanism altitude distribution; So form aspidelite type carrier more easily; Simultaneous oxidation chromium gets in the lattice more and goes, and the product after the calcining makes particle diameter D through refinement
90Reach 3～5mm, as crystal seed, the activity of crystal seed for preparing like this is higher, is used to prepare the agate red colorant; Because preparation agate red colorant must be through multiple crystal conversion when high-temperature calcination, the superfine crystal seed of this particle diameter serves as the crystalline nucleus to the inducing action that rises of crystalline transformation after the adding; Nucleus is slowly grown up again, generates the crystal formation consistent with crystal seed, thereby makes material generate aspidelite type crystal structure carrier more; Chromium ion can get in the lattice more simultaneously, makes color development strengthen, because aspidelite type carrier is completely synthetic; So high thermal resistance is good, red scale value is high, and the final stability that makes improves.
Embodiment
Of the present invention being contemplated that: through introduce crystal seed in the preparation process, reduce the synthetic difficulty of colorant, increase the stability of product quality simultaneously, it is stronger to make it in ceramic colour glaze color development, and color and luster is bright, and resistance to elevated temperatures is good.
In order to make those skilled in the art understand technical scheme of the present invention better, below in conjunction with the present invention being done further detailed description through concrete embodiment.
The agate red ceramic pigment preparation method of introducing crystal seed of the present invention comprises two big steps, i.e. the preparation of synthetic, the colorant of crystal seed is specific as follows:
1, crystal seed preparation
With lime carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes, mixture; With mixture and agate ballstone, water by 100: (450～550): the weight ratio of (54～66) is mixed, is ground, and reaches D until particle diameter
90≤5um, the mixture after will grinding again carries out drying, sieves, and then adds the boric acid account for gross weight 3%～5%, and mixing is then calcined, is ground, drying, obtains crystal seed;
2, colorant preparation
With lime carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes; Add again account for gross weight 1%-3%, the crystal seed that makes in the step 1) and the boric acid that accounts for gross weight 3%～5%; Calcining behind the mixing, grinding, drying get product.
Agate red ceramic pigment by above preparation method makes has following characteristic:
Outward appearance: red-purple powder;
Lightness: 46≤L≤54;
Form and aspect: 24≤a≤29;
Form and aspect :-3≤b≤13.
Embodiments of the invention are following:
Embodiment one
1, crystal seed preparation:
1) with lime carbonate, tindioxide, quartz, chrome green 1: 1: 1 in molar ratio: 0.125 preparation mixes;
2) press said mixture: the agate ballstone: water=100: 500: 60; About 72 hours of ball mill ball milling, particle diameter reaches D behind the ball milling
90≤5um;
3) said mixture is dry in the temperature environment below 150 ℃, make dried mixture water ratio＜0.5%; Dry thing is crossed 325 eye mesh screens;
4) being 99% boric acid with mixture after above-mentioned the sieving and concentration mixes and stirs by 96.5: 3.5 mass ratio;
5) with the said mixture potcal pot calcination of packing into, the incinerating processing condition are: 30 ℃-500 ℃, and intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1250, intensification 5H; 1250 ℃ of following constant temperature 5H, cooling naturally;
6) with above-mentioned calcine ball milling, particle diameter D
90Reach 3-5um, dry (≤150 ℃) are crossed 325 eye mesh screens, are the crystal seed finished product, and are subsequent use;
2, colorant preparation:
1) with lime carbonate, tindioxide, quartz, chrome green 1: 1: 1 in molar ratio: 0.125 mixes;
2) adding crystal seed that step 1 makes and concentration again is that 99% boric acid mixes, and the add-on of crystal seed accounts for crystal seed and boric acid adds 3% of back mixture total weight amount, and the add-on of boric acid accounts for crystal seed and boric acid adds 3.5% of back mixture total weight amount;
3) with pack into 30 ℃～500 ℃ of potcal pot calcinations of said mixture, intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1200 ℃, intensification 3H; 1200 ℃ of following constant temperature 4H, cooling is unloaded below 200 ℃ naturally.
4) with above-mentioned calcine ball milling, particle diameter D90 is controlled at 16um～18um, and dry (≤150 ℃) are crossed 250 eye mesh screens, promptly get the agate red ceramic pigment.
The above agate red ceramic pigment that obtains is carried out fineness and color development detection, and detected result is following:
1, fineness detects
Test gained data: the fineness of agate red ceramic pigment is D
90: 16.8um.
2, color development comparison and detection
The employed glaze colours of agate red ceramic pigment basis glaze formula:
0.276K
2O 0.003Fe
2O
3 3.5SiO
2
0.066Na
2O 0.522Al
2O
3 0.658CaO
Among the present invention, in parent glaze, add massfraction and be the colorant product that does not add crystal seed in 5% synthetic colorant of the present invention and the prior art and do the color development contrast, be labeled as A and B respectively; Temperature of glaze firing is 1100 ℃; Firing time is 60 minutes, soaking time 15-30 minute, and the test color difference:
Test gained data: A sample: L:48.51 a:26.87 b:10.64.
Test gained data: B sample: L:50.34 a:21.56 b:8.99
Above data declaration present embodiment is dark through the agate red ceramic pigment color development that adds the crystal seed preparation, and red scale value is high, and quality improves about 20%.
Embodiment two
1, crystal seed preparation:
1) with lime carbonate, tindioxide, quartz, chrome green 1: 1: 1 in molar ratio: 0.125 preparation mixes;
2) press said mixture: the agate ballstone: water=100: 500: 60; About 78 hours of ball mill ball milling, particle diameter reaches D behind the ball milling
90≤5um;
3) said mixture is dry in the temperature environment below 150 ℃, make dried mixture water ratio＜0.5%; Dry thing is crossed 325 eye mesh screens;
4) being 99% boric acid with mixture after above-mentioned the sieving and concentration mixes and stirs by 95: 5 mass ratio;
5) with the said mixture potcal pot calcination of packing into, the incinerating processing condition are: 30 ℃-500 ℃, and intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1300 ℃, intensification 5H; 1300 ℃ of following constant temperature 5H, cooling naturally;
6) with above-mentioned calcine ball milling, particle diameter D
90Reach 3-5um, dry (≤150 ℃) are crossed 325 eye mesh screens, are the crystal seed finished product, and are subsequent use;
2, colorant preparation:
1) with lime carbonate, tindioxide, quartz, chrome green 1.1: 1.1: 1 in molar ratio: 0.115 mixes;
2) adding crystal seed that step 1 makes and concentration again is 99% boric acid, mixes, and the add-on of crystal seed accounts for crystal seed and boric acid adds 5% of back mixture total weight amount, and the add-on of boric acid accounts for crystal seed and boric acid adds 4% of back mixture total weight amount;
3) with pack into 30 ℃～500 ℃ of potcal pot calcinations of said mixture, intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1200 ℃, intensification 3H; 1200 ℃ of constant temperature 4H, cooling is unloaded below 200 ℃ naturally.
4) with above-mentioned calcine ball milling, particle diameter D90 is controlled at 16um～18um, and dry (≤150 ℃) are crossed 250 eye mesh screens, promptly get the agate red ceramic pigment.
The above agate red ceramic pigment that obtains is carried out fineness and color development detection, and detected result is following:
1, fineness detects
Test gained data: the fineness of agate red ceramic pigment is D
90: 16.8um.
2, color development comparison and detection
The employed glaze colours of agate red ceramic pigment basis glaze formula:
0.216K
2O 0.003Fe
2O
3 3.5SiO
2
0.036Na
2O 0.622Al
2O
3 0.658CaO
Among the present invention, in parent glaze, adding massfraction is that 5% synthetic colorant of the present invention and the product that does not add crystal seed are done the color development contrast, is labeled as C and D respectively; Temperature of glaze firing is 1200 ℃; Firing time is 60 minutes, soaking time 15-30 minute, and the test color difference:
Test gained data: C sample: L:49.61 a:27.87 b:11.62.
Test gained data: D sample: L:53.51 a:15.26 b:18.12.
Above data declaration present embodiment can be stablized color development through the agate red ceramic pigment that adds the crystal seed preparation under the high temperature service condition; More synthetic aspidelite N-type waferN; Resistance to elevated temperatures is good, and the D sample color development that does not add crystal seed preparation fades the color development poor stability.
Embodiment three
1, crystal seed preparation:
1) with lime carbonate, tindioxide, quartz, chrome green 0.9: 1.1: 1 in molar ratio: 0.135 preparation mixes;
2) press said mixture and agate ballstone and water and mix by 100: 450: 56 mass ratio, with the ball mill ball milling about 80 hours, particle diameter reached D behind the ball milling
90≤5um;
3) said mixture is dry in the temperature environment below 150 ℃, make dried mixture water ratio＜0.5%; Dry thing is crossed 325 eye mesh screens;
4) being 99% boric acid with mixture after above-mentioned the sieving and concentration mixes and stirs by 95: 5 mass ratio;
5) with the said mixture potcal pot calcination of packing into, the incinerating processing condition are: 30 ℃-500 ℃, and intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1300 ℃, intensification 5H; 1300 ℃ of constant temperature 5H, cooling naturally;
6) with above-mentioned calcine ball milling, particle diameter D
90Reach 3-5um, dry (≤150 ℃) are crossed 325 eye mesh screens, are the crystal seed finished product, and are subsequent use;
2, colorant preparation:
1) with lime carbonate, tindioxide, quartz, chrome green 0.9: 1.1: 1 in molar ratio: 0.135 mixes;
2) adding crystal seed that step 1 makes and concentration again is 99% boric acid, mixes, and the add-on of crystal seed accounts for crystal seed and boric acid adds 4% of back mixture total weight amount, and the add-on of boric acid accounts for crystal seed and boric acid adds 3.5% of back mixture total weight amount;
3) with pack into 30 ℃～500 ℃ of potcal pot calcinations of said mixture, intensification 4H; 500 ℃-1000 ℃, intensification 4H; 1000 ℃-1200 ℃, intensification 3H; 1200 ℃ of constant temperature 4H, cooling is unloaded below 200 ℃ naturally.
4) with above-mentioned calcine ball milling, particle diameter D90 is controlled at 16um～18um, and dry (≤150 ℃) are crossed 250 eye mesh screens, promptly get the agate red ceramic pigment.
The above agate red ceramic pigment that obtains is carried out fineness and color development detection, and detected result is following:
1, fineness detects
Test gained data: the fineness of agate red ceramic pigment is D
90: 16.8um.
2, color development detects
The employed glaze colours of agate red ceramic pigment basis glaze formula:
0.206K
2O 0.003Fe
2O
3 3.2SiO
2 0.712ZnO
0.036Na
2O 0.42Al
2O
3 ?0.621CaO
Among the present invention, in parent glaze, adding massfraction is that 5% synthetic colorant of the present invention and the product that does not add crystal seed are done the color development contrast, is labeled as E and F respectively; Temperature of glaze firing is 1100 ℃; Firing time is 60 minutes, soaking time 15-30 minute, and the test color difference:
Test gained data: E sample: L:50.31 a:27.87 b:10.64.
Test gained data: F sample: L:48.31 a:16.82 b:9.54.
The zinc oxide reaction that unsettled aspidelite type colorant can occur when in containing the high glaze of zinc, using in chromium stripping and the glaze causes the colorant color development partially secretly green partially, and red scale value reduces.Above data can find out that the agate red ceramic pigment that present embodiment obtains can stablize color development in containing the high glaze of zinc; Red scale value is high; Synthetic aspidelite type carrier colorant fully and can stable existence, and it is dark not add the of the prior art common agate red colorant F sample color development of crystal seed, red scale value is low; Reaction has taken place and has caused color development unstable in instability, chromium ion in the lattice and zinc oxide.
Can find out by the color development data; The agate red colorant that the preparation method of present embodiment makes can be stablized color development under high-temperature condition; Color development is limpid simultaneously, red scale value is high; Synthetic aspidelite type carrier can stable existence when containing the high glaze of zinc and use, and the chromium ion stripping can not occur and causes color development unstable.
More than the present invention has been carried out detailed introduction, use concrete example in the literary composition principle of the present invention and embodiment set forth, the explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
Claims (10)
1. a preparation method who introduces the agate red ceramic pigment of crystal seed is characterized in that, comprises the steps:
1) crystal seed preparation:
With lime carbonate, tindioxide, quartz, inscription green in molar ratio (0.9～1.1): (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes, mixture; With mixture and agate ballstone, water by 100: (450～550): the weight ratio of (54～66) is mixed, is ground, and reaches D until particle diameter
90≤5um, the mixture after will grinding again carries out drying, sieves, and then adds the boron-containing compound mixing account for gross weight 3%～5%, then calcines, grinds, drying, obtains crystal seed;
2) colorant preparation:
With lime carbonate, tindioxide, quartz, chrome green (0.9～1.1) in molar ratio: (0.9～1.1): (0.9～1.1): (0.115～0.135) mixes; Add the boron-containing compound that accounts for crystal seed gross weight 1%-3%, that step 1) makes and account for gross weight 3%～5% again; Calcining behind the mixing, grinding, drying get product.
2. preparation method as claimed in claim 1 is characterized in that step 1) and step 2) in, the mol ratio of lime carbonate, tindioxide, quartz, chrome green is 1: 1: 1: 0.125.
3. preparation method as claimed in claim 1 is characterized in that step 1) and step 2) in the ball milling of grinding for adopting ball mill to carry out.
4. preparation method as claimed in claim 1 is characterized in that, the incinerating processing condition are in the step 1): 30 ℃～500 ℃, and intensification 4H; 500 ℃～1000 ℃, intensification 4H; 1000 ℃～(1200-1300 ℃), intensification 5H; At 1200 ℃～1300 ℃ following constant temperature 5H, cooling naturally then.
5. preparation method as claimed in claim 1 is characterized in that step 2) in the incinerating processing condition be: 30 ℃～500 ℃, intensification 4H; 500 ℃～1000 ℃, intensification 4H; 1000 ℃～1200 ℃, intensification 3H; 1200 ℃ of following constant temperature 4H then are cooled to below 200 ℃ naturally.
6. preparation method as claimed in claim 1 is characterized in that step 1), step 2) in drying all carrying out below 150 ℃.
7. preparation method as claimed in claim 1 is characterized in that step 1) and step 2) in, the water ratio of dry back mixture is less than 0.5%.
8. preparation method as claimed in claim 1 is characterized in that, in the step 1), calcine is ground to particle diameter D in the calcining back
90Reach 3～5mm.
9. preparation method as claimed in claim 1 is characterized in that step 2) in, calcine is ground to particle diameter D in the calcining back
90Be 16mm～20mm.
10. an agate red ceramic pigment is characterized in that, is made by the preparation method in the claim 1～9.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992807A (en) * | 2012-11-26 | 2013-03-27 | 孙志勤 | Method for preparing agate red ceramic glazing material |
| CN103145453A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Praseodymium yellow material for ceramic ink and preparation method thereof |
| CN103145452A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Red colorant for ceramic ink and preparation method thereof |
| CN103145447A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Blue inkjet ceramic pigment and preparation method thereof |
| CN116947536A (en) * | 2023-09-18 | 2023-10-27 | 新明珠集团股份有限公司 | Zirconium-free ground glaze, titanium raw material opacified glazed tile and preparation method thereof |
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| CN101012341A (en) * | 2007-02-02 | 2007-08-08 | 陕西科技大学 | Method of preparing chrome-tin red colorant |
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| CN101012341A (en) * | 2007-02-02 | 2007-08-08 | 陕西科技大学 | Method of preparing chrome-tin red colorant |
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| 郑乃章: "铬锡红色料研究的现状与展望", 《中国陶瓷工业》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102992807A (en) * | 2012-11-26 | 2013-03-27 | 孙志勤 | Method for preparing agate red ceramic glazing material |
| CN103145453A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Praseodymium yellow material for ceramic ink and preparation method thereof |
| CN103145452A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Red colorant for ceramic ink and preparation method thereof |
| CN103145447A (en) * | 2013-03-29 | 2013-06-12 | 佛山市南海万兴材料科技有限公司 | Blue inkjet ceramic pigment and preparation method thereof |
| CN103145447B (en) * | 2013-03-29 | 2014-07-09 | 佛山市南海万兴材料科技有限公司 | Blue inkjet ceramic pigment and preparation method thereof |
| CN116947536A (en) * | 2023-09-18 | 2023-10-27 | 新明珠集团股份有限公司 | Zirconium-free ground glaze, titanium raw material opacified glazed tile and preparation method thereof |
| CN116947536B (en) * | 2023-09-18 | 2024-02-23 | 新明珠集团股份有限公司 | Zirconium-free ground glaze, titanium raw material opacified glazed tile and preparation method thereof |
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|---|---|
| CN102775192B (en) | 2014-04-16 |
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